反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 105 °C
PROCEDURE
实验过程
A solution of compound 57c (0.90 g, 2.5 mmol) and compound 57b (0.96 g, 3.7 mmol) in DMF (5 mL) was purged with N2. Pd(OAc)2 (67 mg, 0.30 mmol) was added, followed by KOAc (1.1 g, 11 mmol) and PPh3 (73 mg, 0.28 mmol). The resulting mixture was stirred at 105° C. for 1.5 h, and allowed to cool to rt. water (100 mL) was added. The resulting mixture was extracted with DCM (3×50 mL). The combined organic layers were dried over Na2SO4, filtered and concentrated under reduced pressure. The residue obtained was purified by flash column chromatography on silica gel (EtOAc/petroleum ether (1:2-2:1 v/v)) to obtain compound 57d as a yellow solid. Mass Spectrum (LCMS, ESI pos.): Calcd. for C31H30N6O3: 535.2 (M+H). Found: 535.2.
WORKUP
后处理
- temperatureto cool to rt
- extractionThe resulting mixture was extracted with DCM (3×50 mL)
- dry with materialThe combined organic layers were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue obtained
- customwas purified by flash column chromatography on silica gel (EtOAc/petroleum ether (1:2-2:1 v/v))